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Electrochemical Porosity Measurement of Electroless

Nickel Coatings on Ferrous Substrates


Information resulting from AESF Research Project
By L. Das, D-T. Chin, G.L. Evarts & R.L. Zeller III

A non-destructive electrochemical method is used to mea- posed by the pores to a corrosive electrolyte. The method
sure the porosity of electroless nickel (EN) coatings on needs only a few minutes to complete a test, and the measured
steel and gray cast iron. The method is based on determin- porosity may be quantitatively expressed in terms of the
ing the mixed potential of a duplex metal surface consist- fraction of pore area on the coating surface.
ing of an EN coating and the ferrous substrate exposed by In the current study, the electrochemical porosity measure-
the pores in a corrosive electrolyte; the measured poros- ment is further used to examine the effect of substrate
ity is quantitatively expressed in terms of the fraction of preparation, including the surface polishing and electrolytic
pore area on the coating surface. The accuracy of this nickel strike, on the porosity of EN coatings on ferrous alloys.
method is compared to the conventional ferroxyl and salt The morphology of the substrate prior to plating is a key
fog spray tests. The electrochemical technique is found to factor controlling the porosity of EN coatings. The studies by
be more sensitive than the ferroxyl test, and provides the Coussement et al.3 and Deng and Møller 4 indicated that
porosity information comparable to that of the salt fog surface roughness of steel substrate had important conse-
test in a much shorter time without destroying the ap- quences on the EN deposit. They found that the corrosion
pearance of test samples. The electrochemical porosity resistance of EN deposits decreased with increase in surface
measurement is subsequently used to examine the effect roughness of the substrate prior to plating. A study by Kudrak
of substrate preparation, including surface polishing and et al.5 also indicated that the porosity of palladium and gold
an electrolytic nickel strike, on the porosity of EN coating coatings increased with increasing roughness of the substrate
on carbon steel and gray cast iron substrates. It is found surface.
that the porosity of EN coatings decrease with decreasing The corrosion resistance of EN is also affected by the
roughness of the substrate surface. Mechanically polish- formation of nodular deposits. A study by Jones6 has shown
ing the substrates to 1-µm smoothness prior to EN plating that the corrosion resistance of nodular hard chromium de-
eliminates nodular EN deposits and reduces the porosity posits may be improved by decreasing nodule size or elimi-
of the EN coating. Electropolishing of the substrate sur- nating the nodules. Substrate defects, such as inclusions and
face also results in EN deposits with low porosity. An debris on the surface, are the main cause of the formation of
electrolytic nickel strike on carbon steel and gray cast nodules and pores in EN deposits. A previous publication by
iron prior to EN plating decreases the porosity of the EN the authors7 revealed that non-catalytic graphite present in
coating by covering exposed graphite and other non- the microstructure of ferrous alloys was responsible for the
catalytic inclusions on the substrate surface with a cata- formation of pores in EN deposits. Electroless nickel deposits
lytic nickel layer. The porosity of an EN coating decreases on nickel substrates, on the other hand, are nodule-free.
with increasing thickness of the nickel strike. A nickel Nickel is catalytic to EN deposition and the EN coating
strike of 1 µm in thickness virtually eliminates nodular initiates and grows uniformly over the entire substrate sur-
EN deposits and reduces the coating porosity by a factor face. Accordingly, a thin nickel strike to cover graphite and
of 100 to an area fraction of pores less than 10-5. other passive inclusions in ferrous substrates prior to EN
plating may potentially reduce the probability of pore forma-
Electroless nickel (EN) coatings are used in engineering tion on EN coatings. The current study was undertaken to
applications to provide protection to ferrous alloys exposed examine the effect of substrate surface polishing and electro-
to corrosive environments.1 Electroless nickel coating on a lytic nickel strike on the porosity of EN coatings using the
ferrous substrate is an example of a more noble coating on a electrochemical porosity measurement.
less noble substrate. If the less noble substrate is exposed to
a corrosive environment through pores and discontinuities in Experimental Procedure
the coating, corrosion of the substrate leading to failure of the Substrates and Surface Preparation Prior to EN
coating would take place. For EN coatings to function satis- Plating
factorily as a corrosion barrier, it is necessary to be free of Three different ferrous substrates were used: (1) AISI 1010
pores. carbon steel containing 0.1 percent carbon; (2) AISI 1075
The porosity of EN coatings is usually measured using the carbon steel containing 0.75 percent carbon; and (3) a gray
ferroxyl test or the salt fog test.2 Although these methods are cast iron containing 3 percent carbon and 2.7 percent silicon.
useful for detecting pores in the deposit, their test results are To examine the effect of substrate polishing on the poros-
not always reproducible. The salt fog test is destructive to the ity of EN deposits, five different types of surface finishes
coating and requires 24 to 48 hr to complete. The purpose of were prepared for the AISI 1010 carbon steel and gray cast
this study is to develop a fast and non-destructive method to iron coupons. They were: (1) as received from a commercial
measure the porosity of EN coatings on ferrous substrates. metal sample supplier; (2) polished with 120-grit silicon
The method is based on an electrochemical principle of carbide paper; (3) polished with 600-grit silicon carbide
measuring the mixed potential of a duplex metal surface paper; (4) polished with 1-µm alumina paste; and (5)
consisting of the EN coating and the ferrous substrate ex- electropolished. Electropolishing of the carbon steel was

66 PLATING & SURFACE FINISHING


carried out in an electrolyte composed of 75 percent by an example of a noble coating on an active metal with low
volume of phosphoric acid (85 wt percent in concentration) porosity. In a corrosive electrolyte, the anodic area is the
and 25 percent by volume of lactic acid (85 wt percent in ferrous substrate exposed through the pores and the cathodic
concentration) at 25 A/dm2 and 60 o C for 30 min.8 area is the EN coating. Accordingly, the above principle for
Electropolishing of the gray cast iron was performed in a porosity measurement is applicable. If a calibration plot in
solution containing 94 percent by volume of glacial acetic the form of area fraction of exposed iron vs. corrosion
acid and 6 percent by volume of perchloric acid (60 wt potential is available, the porosity of an EN coating on a
percent in concentration) at 0 oC and a cell voltage of 40 V for ferrous substrate may be determined from the calibration plot
a period of 5 min.8 by measuring the corrosion potential of the EN-coated sample.
A nickel strike on some carbon steel and cast iron coupons In this study, a galvanically connected EN-iron couple was
prior to EN plating was carried out with a Wood’s bath used to calibrate the change in corrosion potential as a
composed of 240 g/L of nickel chloride and 384 g/L of function of the area fraction of iron. Because the galvanic
hydrochloric acid. The substrates were mechanically pol- corrosion potential depends on the type and composition of
ished to a 600-grit surface finish prior to the strike. Platinum the EN deposit, two different EN sheets were used for the
was used as the anode and a cathodic current density of 6 A/ calibration. The first was prepared by depositing 67.5 µm of
dm2 was maintained during the strike. The strike was carried high-phosphorus EN (89.5 wt % Ni, 10.5 wt % P) on a large
out for 2, 5 and 10 min to yield nickel coatings of different nickel sheet, 64 cm2 in surface area, from the commercial EN
thickness. bath, while the second was prepared by depositing 30 µm of
EN (90.3 wt % Ni, 9.7 wt % P) on another nickel sheet of the
EN Coatings for Porosity Measurement same surface area from the generic EN bath. An iron wire
Two types of EN coatings were used. The first EN coating (0.25 mm in dia.), insulated with wax except at the tip, was
(89.5% Ni, 10.5% P) was prepared using a commercial bath. galvanically connected to the EN-plated nickel sheet. The
To prepare the samples for porosity measurements, AISI area ratio of the iron wire to EN coating was varied by
1010 carbon steel coupons were soaked in a commercial changing the length of the exposed iron tip. The corrosion
cleaning solution, electrocleaned with periodic reverse cur- potential of this EN-iron couple was measured in a solution
rent, activated by acid dip in 37-percent HCl, and immersed containing 3 wt percent NaCl and 1.5 wt percent H2O2 at 23
o
in the commercial EN bath. The substrates were then plated C , as described by Shome and Evans.10 A saturated calomel
for various lengths of time to yield EN coating thicknesses of electrode (SCE) was used as the reference, and the corrosion
0.4 to 64 µm. These samples were tested for porosity using potential of the EN-iron couple was measured with a high
the electrochemical technique as well as with conventional input impedance electrometer.a The results of the calibration
ferroxyl and salt fog tests. are shown in Fig. 1. It was noted that the calibration lines for
The second type of EN coating (90.3% Ni, 9.7% P) was the commercial and generic EN have a different slope and
prepared by dipping the ferrous substrates in a generic EN intercept. Because the phosphorus content in the two coatings
bath containing 44 g/L nickel sulfate hexahydrate, 10 g/L was nearly the same, this suggests that additives used in the
sodium hypophosphite hydrate, 42 g/L aminoacetic acid and commercial bath significantly modified the electrochemical
10 g/L acetic acid at 88 oC and pH 4.5. The ferrous coupons properties of the EN deposit.
were polished to various degrees of roughness. They were To measure the porosity of a ferrous substrate coated with
anodically electrocleaned in 1 M NaOH at 5 A/dm2 for 2-3 EN, the sample was immersed in the same electrolyte at 23 oC
min and were activated by dipping in 37-percent HCl for 1 and its corrosion potential measured with reference to the
min. The EN plating was carried out in the generic bath for SCE. The area fraction of pores corresponding to the mea-
different time intervals to produce coating thicknesses rang- sured corrosion potential was then determined from the
ing from 2 to 35 µm. The morphology of the EN-coated calibration plot.
samples was observed under a scanning electron microscope
(SEM), and the coating porosity was measured using the Ferroxyl Test
electrochemical technique. The porosity measurement using the ferroxyl test was carried
out in accordance with ASTM B733 (1994). The test solution
Electrochemical Porosity Measurement
The principle of the electrochemical porosity measurements
is based on the fact that a duplex metal surface (part coating
Porosity, area fraction (x 103)

and part substrate exposed through pores in the coating)


exhibits a corrosion potential on exposure to a corroding
electrolyte. The value of the corrosion potential depends on
the area fraction of pores and the polarization of the anode
(base metal) and cathode (coating). An equation by Mansfeld9
for the corrosion potential Ecorr of a galvanic couple where the
anodic area is much smaller than the cathodic area may be
given as:
Ecorr = k - [b abc/(ba + bc)] log (θA)

where θA is the area fraction of the anode (or porosity); ba is


the Tafel slope for the anodic reaction; bc is the Tafel slope for
the cathodic reaction; and k is a constant. This equation Corrosion potential, V (vs. SCE)
indicates that a plot of the corrosion potential vs. log θA would Fig. 1—Calibration plot for area fraction of pores on EN coating vs.
yield a straight line. Electroless nickel on ferrous substrate is corrosion potential of EN-coated ferrous substrate.

July 1997 67
with 2.1 µm of EN deposited; it
Table 1 was unable to detect pores in
Comparison of Electrochemical Porosity Measurement thicker coatings. The salt fog
With Results of Ferroxyl & Salt Fog Tests tests, on the other hand, were
successful in detecting pores
on all the samples, shown by
Porosity the presence of rust spots on the
sample surface. The number of
EN Deposit Ferroxyl Salt Fog Electrochemical Estimated pores decreased with increas-
Thickness Test Test Test Pore Size* ing in coating thickness, as
:m (no. of pores on (no. of pores on (area fraction (µm) shown in Table 1. The electro-
8 cm2 sample 8 cm2 sample of pores) chemical tests were capable of
area) area) measuring the area fraction of
0.42 - - 2.0 x 10-3 - pores on EN coatings.
The porosity of the commer-
cial EN coating was plotted
1.05 - - 1.9 x 10-3 - against deposit thickness in Fig.
2. The results obtained with salt
-3
fog tests agreed with the results
2.1 11 156 1.4 x 10 96 of electrochemical porosity
measurements. The porosity of
6.4 0 61 1.3 x 10 -3
147 EN on steel decreased with in-
crease in deposit thickness in
the range of 0-30 µm, beyond
26 0 3 0.93 x 10-3 560 which the porosity remained
approximately constant. The
electrochemical technique
38 0 5 0.97 x 10-3 440 gives results comparable to
those of the salt fog tests and
-3 requires a much shorter time
51 0 2 0.95 x 10 700
without destroying the sample.
The salt fog test and electro-
64 0 1 0.94 x 10 -3
980 chemical porosity measurement
data can be combined to esti-
* Estimated from the results in Columns 3 and 4, using the formula: mate the average pore size
4 (area fraction of pores) (sample area) present on the EN coating. The
Average pore diameter=
π number of pores estimated results are listed in
the last column of Table 1. It is
was prepared by dissolving 25 g potassium ferricyanide and noted that the average pore size
15 g sodium chloride in 1 L of distilled water. The test increases in a linear fashion with an increase in coating
samples were cleaned and immersed in the test solution for 30 thickness. This suggests that during the EN deposition pro-
o
sec at 25 C. The samples were then rinsed in water, dried in cess, small pores were being filled with EN, with only large
air, and examined for blue ferrous ferricyanide formed at the pores expected after a thick EN coating was deposited.
pore sites. The porosity of EN coatings on AISI 1010 and 1075 carbon
steel, prepared from the generic EN bath, is shown in Fig. 3.
Salt Fog Test The porosity of EN coatings on both substrates decreased
The salt fog test was carried out in accordance with ASTM with increasing deposit thickness. The porosity was slightly
B117 (1994). The EN-coated specimens were cleaned and lower on AISI 1010 steel than on AISI 1075 steel when
exposed in a salt spray chamber for 24 hr. The salt solution coating thickness was less than 10 µm. This may be a result
was 5-percent sodium chloride in distilled water. The tem- of the fact that AISI 1075 steel contains more carbon in its
perature in the salt spray chamber was maintained at 35 oC. microstructure than AISI 1010 steel.
After exposure, the test samples were rinsed in water to
remove salt deposits, dried and examined for rust spots on the Substrate Surface Roughness & Porosity of EN
surface. Coating
The effect of substrate roughness on EN porosity was tested
Results and Discussion with AISI 1010 carbon steel and gray cast iron coupons. They
Comparison of Ferroxyl, Salt Fog, & were polished to various roughnesses and coated with EN in
Electrochemical Porosity Measurements the generic bath to a common thickness of 12 ±0.7 µm.
Table 1 summarizes the results of the ferroxyl, salt fog, and Coating porosity was then measured with the electrochemi-
electrochemical porosity measurements for various thick- cal technique. Table 2 lists the porosity of generic EN
nesses of the commercial EN coating. With ferroxyl tests, coatings on the carbon steel and gray cast iron with different
blue spots appeared at the location of pores. The ferroxyl test surface roughness. For AISI 1010 carbon steel, the porosity
showed positive identification of pores only on the substrate of EN coatings on the as-received substrate surface and on the

68 PLATING & SURFACE FINISHING


Table 2

Porosity, area fraction (x 103)


Effect of Substrate Roughness on Porosity
of Generic EN Deposit

Type of Substrate Porosity (Area Fraction of Pores)


Surface Finish

AISI 1010 Steel Gray Cast Iron

Blast with glass 3.5 x 10-3 -


beads (as received)

120-grit 3.2 x 10-3 4.0 x 10-3

Deposit thickness, µm 400-grit - 2.3 x 10-3

600-grit 1.2 x 10-3 1.4 x 10-3

1-µm alumina 0.67 x 10-3 1.3 x 10-3


paste

0.75 x 10-3 0.9 x 10-3


Number of pores

Electrochemical
polish

Porosity, area fraction (x 103)

Deposit thickness, µm
Fig. 2— Porosity of commercial EN coating on AISI 1010 carbon steel as
function of coating thickness: (a) results of electrochemical measurement;
(b) results of salt fog test.

120-grit finish were higher than that on the 600-grit surface


finish. The porosity of EN coating on the substrates polished
with 1-µm alumina paste and electropolishing was the low-
est. For the gray cast iron substrates, the porosity was reduced Thickness of EN deposit, µm
by half when the surface roughness decreased from 120-grit
to a 600-grit finish prior to EN plating. Mechanical polishing Fig. 3—Porosity of generic EN coating on AISI 1010 and 1075 carbon
to 1 µm in smoothness and electropolishing further reduced steel as function of coating thickness by electrochemical technique.
the porosity. coating on electropolished AISI 1010 carbon steel, as shown
Figure 4 is a SEM photomicrograph showing the morphol- in Table 2.
ogy of EN deposit on the as-received surface of an AISI 1010 The SEM examination of EN coatings on gray cast iron
carbon steel coupon. Figure 5 is a SEM photomicrograph of coupons with different surface finishes (120-grit, 400-grit,
EN deposit on a carbon steel coupon polished to 1 µm 600-grit, 1µm, and electropolish) revealed the presence of
smoothness prior to EN plating. The inset in each photomi- nodular deposits on all the samples. The nodules were ob-
crograph shows the substrate surface prior to EN deposition. served along the grinding marks on the coupons with 120-
The EN on the as-received steel coupon was nodular in grit, 400-grit and 600-grit finish. When the gray cast iron was
structure. The size of nodules was found to decrease with polished to 1 µm in smoothness, the graphite flakes present
decreasing surface roughness and, when the substrate surface in the microstructure showed up on the surface as shown in
was polished to 1 µm in smoothness, the EN deposit became Fig. 6a. Figure 6b shows that the nodular EN deposit was
free of nodules, as shown in Fig. 5. Small nodules were formed on the graphite inclusion, whereas the EN deposit on
observed on the EN deposit on the electropolished steel the surrounding iron portion of the substrate was free of
surface. The electropolished steel surface was passive to EN nodules.
deposition and had to be activated by etching in 37-percent
HCl for a longer period of time. The etching in HCl may have Effect of Nickel Strike on the Porosity of EN
destroyed the surface smoothness and caused the formation Deposits
of small nodules and a slight increase in the porosity of the EN The results in the previous section show that surface rough-

July 1997 71
Table 3
Effect of Electrolytic Nickel Strike Prior to
Plating on Porosity of Generic EN Deposit
On Carbon Steel & Gray Cast Iron

Substrate Nickel Strike Nickel Porosity


Time Strike (Area Fraction
(min) Thickness of Pores)
(µm)

ISI 1010 0 0 1.2x10-3


Carbon Steel

2 0.25 0.47x10-3
Fig. 5—SEM photomicrograph of generic EN deposit (12 µm thick) on an
-5 AISI 1010 carbon steel coupon; surface mechanically polished to 1 µm
5 0.46 < 10 smoothness (inset) prior to EN plating.

Gray Cast Iron 0 0 1.4x10-3


(a) (b)
-3
2 0.22 1.7x10

5 0.45 0.9x10-3

10 0.97 < 10-5

Fig. 6—SEM photomicrograph of gray cast iron coupon polished to 1 µm


smoothness: (a) before EN plating; (b) after coating with 12 µm generic
EN.

(a) (b)

Fig. 4—SEM photomicrograph of generic EN deposit (12 µm thick) on the


as-received surface (without any polishing) of an AISI 1010 carbon steel
coupon. The inset shows the surface prior to EN plating.

ness of the substrate affects the porosity of the EN deposit.


The presence of graphite flakes on gray cast iron surfaces also
results in nodular EN deposits with an increased porosity. One
way to reduce the porosity of EN coating on ferrous substrates
Fig. 7—SEM photomicrograph of gray cast iron coupon pre-coated with
is to cover exposed graphite and other non-catalytic surface 0.2 µm of an electrolytic nickel strike: (a) before EN plating; (b) after
inclusions with a thin layer of electrolytic nickel. Experi- coating with 12 µm generic EN.
ments were carried out to determine the effectiveness of
electrolytic nickel strikes prior to EN plating in reducing the to cover all the graphite flakes present on the surface of gray
porosity of EN deposit on AISI 1010 carbon steel and gray cast iron. The EN deposit still exhibited a nodular structure,
cast iron coupons having a 600-grit surface finish. Figures 7a as shown in Fig. 7b. Two min of nickel strike eliminated
and 8a show the surface of gray cast iron coupons after 2 min nodular deposits on AISI 1010 carbon steel, however. When
(0.2 µm coating thickness) and 10 min (1 µm coating thick- the nickel strike time was increased to 10 min, all the graphite
ness) nickel strike, respectively. Figures 7b and 8b are the flakes on gray cast iron were covered by the electrolytic
SEM photomicrographs of the same coupons coated with 12 nickel coating, and the subsequent EN coating became free of
±0.7 µm of EN. Two min of nickel strike was not long enough nodules, as seen in Fig. 8b.

72 PLATING & SURFACE FINISHING


(a) (b)
References
1. ASTM B 733-90, Standard Specification for Auto-cata-
lytic Nickel-Phosphorus Coatings on Metals, American
Society for Testing Materials, Philadelphia, PA, 1994.
2. ASTM B 117-94, Standard Practice for Operating Salt
Spray (Fog) Testing Apparatus, American Society for
Testing Materials, Philadelphia, PA, 1994.
3. M.J. Coussement, P. Jensen, J.R. Roos, J.P. Celis and M.
Neutjens, “Results of Research Work with NiSO4,” Elec-
troless Nickel Conf. IV (1985).
4. H. Deng, and P. Møller, Proc. AESF Annual Tech. Conf.,
Anaheim, CA, 979 (1993).
5. E.J. Kudrak, J.A. Abys and F. Humiec, ibid., 84, 32 (Jan.
1997).
Fig. 8—SEM photomicrograph of gray cast iron coupon pre-coated with 1 6. A.R. Jones, Plat. and Surf. Fin., 81, 14 (Oct. 1994).
µm of an electrolytic nickel strike: (a) before EN plating; (b) after coating 7. L. Das, D-T. Chin, R.L. Zeller, and G.L. Evarts, Plat.
with 12 µm generic EN.
and Surf. Fin., 82, 56 (Oct. 1995).
The EN-coated carbon steel and gray cast iron coupons, 8. P. Dettner, in Electrolytic and Chemical Polishing of
pre-coated with an electrolytic nickel strike, were tested for Metals, Needer Press, Tel Aviv, 1988.
porosity using the electrochemical porosity measurement. 9. F. Mansfeld, Corrosion, 27, 436 (1971).
Table 3 lists the porosity of EN deposits on the substrates with 10. S.C. Shome and U.R. Evans, J. Electrodep. Tech. Soc.,
different nickel-strike thickness. The porosity of EN on both 27, 65 (1951).
gray cast iron and steel substrates decreased with an increase
in the thickness of the nickel strike. Without a nickel strike,
the area fractions of pores of EN was on the order of 10-3.
When the thickness of the nickel strike was 1 µm, the porosity
of the EN coating on both AISI 1010 carbon steel and gray
cast iron was reduced to less than 10-5 (area fraction of pores).

Summary
1. The results of porosity measurements of EN coatings on
steel substrate using the electrochemical, conventional Das Chin Evarts Zeller
ferroxyl and salt fog spray techniques indicate that the
electrochemical technique is a quick and quantitative About the Authors
method for measuring EN porosity in the form of area Dr. Leena Das is a member of the R&D staff at Frederick
fractions of pores on the coating surface. The electro- Gumm Chemical Co., 538 Forest St., Kearny, NJ 07032. Her
chemical method is more sensitive than the ferroxyl test, research interests are electroless nickel and chloride zinc
and provides porosity information comparable to that plating. She received a B. Tech in chemical engineering from
obtained with the salt fog spray test in a much shorter time the Indian Institute of Technology, Kharagpur, and MS and
without destroying the appearance of test samples. PhD in chemical engineering from Clarkson University.
2. The porosity of EN coatings on carbon steel and gray cast Dr. Der-Tau Chin is professor of chemical engineering,
iron substrates decreases with decreasing roughness of Clarkson University, Potsdam, NY 13699. He has more than
the substrate surface. Mechanically polishing the sub- 20 years’ research experience in electroplating, corrosion,
strates to 1 µm smoothness prior to EN plating eliminates electrochemical energy conversion, and industrial electro-
nodular EN deposits and reduces the porosity of the EN lytic processes. Prior to joining Clarkson, he was a senior
coating. Electropolishing of the ferrous substrates also research engineer in the Electrochemistry Department of
results in EN deposits with a low porosity. General Motors Research Laboratories. Dr. Chin received
3. An electrolytic nickel strike on carbon steel and gray cast his PhD from the University of Pennsylvania.
iron prior to EN plating decreases the porosity of EN Gerald L. Evarts is a technical service engineer with
coating by covering exposed graphite and other non- Occidental Chemical Corp. Tech Center in Niagara Falls,
catalytic inclusions on the substrate surface with a cata- NY. He has worked in the coatings industry for more than 27
lytic nickel layer. The porosity of EN coatings decreases years in various research and technical service positions. He
with increasing thickness of a nickel strike. One µm of has published several papers and holds five patents in the
nickel strike virtually eliminates nodular EN deposits and field of protective coating.
reduces the coating porosity to less than 10-5 (area fraction Dr. Robert L. Zeller III, P.E., is the technical team leader
of pores). for specialty chemicals at the Occidental Chemical Corp.
a
Model 610C, Keithley Instruments, Cleveland, OH Niagara Plant. He holds a BS and an MS in chemical
engineering from the University of Akron and a PhD in
Editor’s note: Although this article is not a formal, chemical engineering from Case Western Reserve Univer-
required report, the work described here was supported by sity. He was recently recognized as a 1994 Inventor of the
AESF Research Project 90. This is an edited version of the Year for a patented process to produce hypophosphorous
paper presented at AESF SUR/FIN® ’97. acid by electrodialysis.

July 1997 73

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